WO2014013709A1 - Partie d'extrémité de porte-échantillon, porte-échantillon présentant ladite partie d'extrémité de porte-échantillon, étage gonio et microscope électronique présentant ledit étage gonio - Google Patents

Partie d'extrémité de porte-échantillon, porte-échantillon présentant ladite partie d'extrémité de porte-échantillon, étage gonio et microscope électronique présentant ledit étage gonio Download PDF

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Publication number
WO2014013709A1
WO2014013709A1 PCT/JP2013/004315 JP2013004315W WO2014013709A1 WO 2014013709 A1 WO2014013709 A1 WO 2014013709A1 JP 2013004315 W JP2013004315 W JP 2013004315W WO 2014013709 A1 WO2014013709 A1 WO 2014013709A1
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WO
WIPO (PCT)
Prior art keywords
sample
sample holder
tip
pressing
present
Prior art date
Application number
PCT/JP2013/004315
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English (en)
Japanese (ja)
Inventor
宮崎　裕也
Original Assignee
株式会社メルビル
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2012158550A external-priority patent/JP5908357B2/ja
Priority claimed from JP2012214258A external-priority patent/JP6137801B2/ja
Application filed by 株式会社メルビル filed Critical 株式会社メルビル
Priority to US14/414,682 priority Critical patent/US9240304B2/en
Publication of WO2014013709A1 publication Critical patent/WO2014013709A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
    • H01J37/185—Means for transferring objects between different enclosures of different pressure or atmosphere
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/261—Details
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/18—Vacuum control means
    • H01J2237/186—Valves
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/2007—Holding mechanisms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20207—Tilt
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20214—Rotation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H01J2237/2802—Transmission microscopes

Definitions

  • the present invention relates to a sample holder tip and a sample holder having the sample holder tip, and more particularly to a sample holder tip having a specific sample pressing means and a sample holder having the sample holder tip.
  • the present invention also relates to a gonio stage and an electron microscope having the gonio stage, and more particularly to a gonio stage having a valve opening / closing mechanism and an electron microscope having the gonio stage.
  • the tip of a sample holder (hereinafter also referred to as a sample cradle) inserted into a limited space between the gaps of the objective pole piece of the transmission electron microscope. ))
  • a sample cradle (hereinafter also referred to as a sample cradle) inserted into a limited space between the gaps of the objective pole piece of the transmission electron microscope. ))
  • a transmission electron microscope will be described as an example.
  • a sample to be observed with a transmission electron microscope is mounted on a sample cradle and observed.
  • the sample cradle needs at least a cradle pedestal and a sample pressing member.
  • the sample presser requires some fixing means for sandwiching the sample mesh in the cradle body, and therefore means for arranging fixing screws is generally used.
  • the thickness of the sample pressing plate and the size of the sample fixing screw must be reduced.
  • M1-M2 size screws are generally used.
  • a sample exchanging device including a sample chamber, a sample exchanging chamber, a gate valve, and a sample exchanging rod is known (Patent Document 1).
  • the sample attachment work is done by contacting the sample as a result of a screwdriver or tweezers accidentally slipping as a result of the screw that is pinched by both skilled and tweezers coming off and losing. In many cases, the sample is destroyed.
  • sample cradle part at the tip of the sample is generally only about 2 mm thick, and when tightening a screw, an expert knows the minimum amount of force to press the TOOL for tightening the screw. If this is done, the TOOL (driver) will be pushed unnecessarily, and as a result, many accidents will occur in which the sample cradle will be bent. Therefore, it is desired to simplify the sample mounting means with a compact design.
  • the sample holder generally has a sample holder for fixing the sample and a fixing screw for fixing the sample holder.
  • the sample mounting method for the standard sample holder is as follows. First, the sample fixing screw is loosened and the screw is removed. Next, after removing the sample holder, a sample mesh is placed on the sample base, a spacer is placed so that the sample mesh is not displaced, and a sample holder is placed thereon so as not to be displaced.
  • the sample is fixed with a sample fixing screw, and a process of tightening the fixing screw with a screwdriver while carefully guiding it to the screw hole with tweezers so that the mesh, spacer, and sample presser do not shift.
  • a spacer is necessary are as follows: When tightening the sample holder with the fixing screw, the sample holder may rotate and damage the sample (bend or contact the surface). Even if the holder rotates by inserting a spacer between the sample and the sample holder 1. It is difficult to damage the sample directly. This is because the sample mesh has various thicknesses and can be used to adjust the thickness.
  • the sample holding means and the fixing means are structurally small parts, so they may be skipped, dropped or lost in the worst case. 2. Due to the complexity of the installation work, the sample and sample holder may be replaced many times. 3. Since the sample may be placed many times, the sample that has been made may be dropped, broken, or pierced with tweezers or a screwdriver. 4. When fixing the fixing screw, it is a very complicated process to hold the fixing screw with tweezers with one hand and tighten with a screwdriver with the other hand. Sometimes the driver or tweezers slip, causing an accident that breaks through the sample mesh. 5. In addition, if the sample is left in the atmosphere for a long time, it may cause contamination and oxidize, so there is a problem that it takes time to install it as quickly as possible. (Originally, vacuum conveyance is ideal.)
  • the valve is opened and closed manually or while rotating the sample holder. That is, in the existing gonio stage (Gonio), the sample holder is inserted, and the portion that was at atmospheric pressure before insertion is preliminarily evacuated. After that, the partition valve that has been cut off from the high vacuum (vacuum of the electron microscope housing) provided on the gonio stage is opened, and the holder is inserted.
  • a spherical valve (partition valve) connected to the valve opening / closing mechanism cylinder is driven by rotating the valve opening / closing mechanism cylinder disposed inside the holding cylinder by rotating the sample holder by 90 ° to 120 °. It is a process to rotate and open.
  • the sample holder is cooled with liquid nitrogen (generally called a cooled sample holder), but it is necessary to rotate the cooled sample holder by 90 ° to 120 °. A situation may occur where liquid nitrogen spills from the container (dewar).
  • the goniometer stage is once rotated and tilted, rotated (rotation angle when inserting the sample holder), the sample holder is inserted straight, and after the preliminary vacuum is drawn, the goniometer stage is returned to its original position. It is necessary to insert it back (see FIGS. 14 and 15). That is, with the partition valve closed, the cooled sample holder is inserted into the goniometer stage with the upper body turned on the shaft so that the liquid nitrogen container (dewar) faces upward. After that, after preliminary exhaust is completed, it is necessary to make the liquid nitrogen container (dewar) face up to turn the partition valve. However, this operation is dangerous, and until the sample holder is loaded It was necessary to stay in place.
  • the present invention has an object to provide a sample holder tip that can be compactly designed and can be easily loaded with a sample, and a sample holder having the sample holder tip.
  • the present invention provides a sample holder tip portion that can be easily loaded with a sample, and a sample holder having the sample holder tip portion. Objective.
  • an object of the present invention is to provide a gonio stage having a valve opening / closing mechanism in order to solve the above problems.
  • the present inventor has analyzed the accident related to the sample exchange of the sample holder, and as a result of intensive studies, has come to find the present invention.
  • the tip of the sample holder includes a sample mounting base, a sample mesh for placing a sample, a sample pressing part for pressing the sample mesh, and a clamp part for clamping the sample pressing part.
  • the sample pressing portion has a ring shape.
  • the side surface of the sample pressing portion has a taper or a convex portion.
  • the sample pressing portion is an abacus ball-shaped ring shape.
  • the clamp portion is clamped by using a taper or a convex portion of a side surface portion of the sample pressing portion.
  • the clamp portion is made of an elastic member.
  • the clamp portion is a spring pin.
  • the sample pressing part has a detaching means for detaching the sample pressing part from the sample holder tip.
  • the detaching means is a groove disposed on the inner diameter side of the ring-shaped member.
  • the detaching tool of the present invention is a detaching tool for detaching the sample pressing portion corresponding to the detaching means of the sample holder tip portion of the present invention.
  • the kit of the present invention is characterized by comprising the tip of the sample holder of the present invention and the detaching tool of the present invention.
  • the sample holder of the present invention is characterized by comprising the tip of the sample holder of the present invention.
  • the present inventor has analyzed the accident relating to the sample exchange of the sample holder, and as a result of intensive studies, has found the present invention.
  • the sample holder tip of the present invention comprises a sample holder comprising a sample mounting base, a sample mesh for placing a sample, a sample pressing means for pressing the sample mesh, and a fixing means for fixing the sample pressing means. It is a front-end
  • the said sample pressing means has an elastic member, It is characterized by the above-mentioned.
  • the sample pressing means is composed of one or more.
  • the sample pressing means is housed in a groove provided in the sample setting base.
  • the sample pressing means is movable in the longitudinal direction of the sample holder.
  • the sample pressing means has a guide groove.
  • the elastic member is a hook.
  • sample holder of the present invention is characterized by comprising the tip of the sample holder of the present invention.
  • the present inventor has intensively studied the attachment mechanism with the gonio stage and the sample holder, and as a result, has found the present invention.
  • the gonio stage of the present invention includes a gate type valve, a guide roller provided in the gate type valve, a first vacuum O-ring provided in the gate type valve, and the gate type valve driving shaft.
  • a valve opening / closing mechanism comprising the valve opening / closing mechanism, wherein the gate valve and the shaft are rotatable by at least one fulcrum. To do.
  • valve opening / closing mechanism further includes a support roller.
  • valve opening / closing mechanism has a tapered portion for guiding the guide roller.
  • the shaft has a second vacuum O-ring.
  • the shaft is in a shaft holding cylinder in a sample holder holding cylinder.
  • the sample holder holding cylinder has a sample holder holding member.
  • the electron microscope of the present invention is characterized by having the goniostage of the present invention.
  • the gonio stage of the present invention it is possible to insert the sample holder without rotating, and thus the insertion while cooling with liquid nitrogen is simplified, and the liquid nitrogen is reduced to zero. It has an advantageous effect of preventing misoperation such as rain.
  • the use of a gate type valve eliminates the need for an operation work by a person to rotate the sample holder after preliminary vacuum evacuation (Pre-pump), so that it is possible to use Auto.
  • the auto operation reduces the staying time in the electron microscope room and has the effect of preventing contamination of the electron microscope room atmosphere due to disturbances such as air flow in the electron microscope room caused by people coming and going. This has the advantageous effect of stabilizing the atmosphere in the observatory.
  • Auto since Auto can be achieved, the time required for inserting the Holder is shortened, and the throughput of the work itself is improved, and the productivity is increased.
  • FIG.1 (a) is sectional drawing which shows a mode that the sample at the time of using the sample holder front-end
  • FIG. 1 (b) shows a cross-sectional view after completion of sample attachment when the sample holder tip is used in one embodiment of the present invention.
  • FIG. 2 is a diagram showing a sample holder tip in one embodiment of the present invention.
  • FIG. 3A shows a conventional standard cradle.
  • FIG. 3B is a diagram showing a cradle in one embodiment of the present invention.
  • FIG. 4 is a schematic diagram of a cradle using a conventional sample pressing plate and fixing screws.
  • FIG. 5 is a diagram showing a procedure for attaching the tip end portion of the sample holder in one embodiment of the present invention.
  • FIG. 6 is a diagram showing a procedure for attaching the tip end portion of the sample holder in one embodiment of the present invention.
  • FIG. 7 is a view showing a perspective view of the tip end portion of the sample holder in one embodiment of the present invention.
  • FIG. 8 is a diagram showing a conventional sample attachment procedure.
  • FIG. 9 is a diagram showing a conventional sample attachment procedure.
  • FIG. 10 shows a conceptual diagram of a basic configuration in an example of a transmission electron microscope applicable in the present invention.
  • FIG. 11 shows an embodiment of a gonio stage in an example of the present invention. The state when the gate type valve is closed is shown.
  • FIG. 12 shows an embodiment of a gonio stage in an example of the present invention.
  • the movement of opening and closing the gate type valve is shown.
  • the trajectory of the opening and closing movement is depicted step by step.
  • FIG. 13 shows an embodiment of a gonio stage in an example of the present invention.
  • the state when the gate type valve is opened is shown.
  • FIG. 14 shows an aspect of a conventional gonio stage. Indicates the state when the valve is closed.
  • FIG. 15 shows an aspect of a conventional gonio stage. Indicates the state when the valve is opened.
  • the tip end portion of the sample holder according to the present invention includes a sample mounting base, a sample mesh for placing the sample, a sample pressing portion for pressing the sample mesh, and a clamp portion for clamping the sample pressing portion.
  • the sample installation pedestal is a pedestal on which a sample is placed.
  • a sample mesh is placed on the sample mounting base, and the sample is placed on the sample mesh.
  • the sample mesh is usually fixed when used in a microscope.
  • the sample mesh is generally fixed to the sample mounting base with screws or the like through the sample pressing plate.
  • it consists of the sample pressing part which presses a sample mesh, and the clamp part which clamps the said sample pressing part. At least a part of the sample pressing part and at least a part of the clamp part have fixing means that can fix the sample pressing part and the clamp part to each other.
  • the sample pressing portion has a ring shape. If it is a theoretical shape without considering the cost, it can be applied to a deformed ring such as a C-shaped ring, a star-shaped ring, and a thread-wound ring.
  • the side surface of the sample pressing part has a taper or a convex part. By using the tapered surface, a groove can be provided on the clamp portion side so that the sample pressing portion can be fixed.
  • the sample pressing portion has an abacus-shaped ring shape. Having a tapered surface in this way has an advantage that it can be easily attached to and detached from the clamp portion.
  • the sample holding part can be fixed by providing a concave part on the clamp part side using the convex part. According to such a design, the sample pressing portion can be fixed to the sample holder without a member such as a screw.
  • the clamp portion is made of an elastic member.
  • the mechanism by which clamping is possible is not particularly limited.
  • a structure in which at least a part or all of the sample pressing part and at least a part or all of the clamping part are engaged with each other, or a hooking structure is used.
  • the sample pressing part can be fixed.
  • the structure that engages or catches can be performed on the contact surface between the sample pressing part and the clamp part.
  • the sample pressing part has a ring shape, the ring-shaped outer peripheral surface and the clamp part What is necessary is just to be able to fix by the structure which meshes between, or the structure caught.
  • the clamp portion is a spring pin.
  • the clamp part is a spring pin
  • the taper can be used to make the sample pressing part and the clamp part easier to attach and detach. Become. That is, by disposing a rod-shaped spring pin on the cradle, using the spring pin, a chevron-shaped protrusion provided on the outer periphery of the ring is accommodated and can be clamped.
  • the abacus protrusion is an abacus bead protrusion when the abacus bead-shaped ring shape is used, the abacus protrusion can be hooked and fixed to the spring pin.
  • two spring pins are used to hold two points of the sample pressing ring.
  • the shape is not particularly limited as long as the sample pressing ring can be held at one point, two points, three points, or more.
  • the inner diameter side expands once from the outer shape of the sample pressing ring, can be expanded to the inner diameter that the sample pressing ring can pass through, and has a deformed ring shape that is plastically (spring-like) and contracts to the inner diameter in the free state. If there is, it is feasible.
  • the sample pressing part has a detaching means for detaching the sample pressing part from the sample holder tip. This is for facilitating the attachment / detachment of the sample pressing portion.
  • the desorption means is not particularly limited as long as it does not interfere with observation with a microscope.
  • the desorption means is a groove disposed on the inner diameter side of the ring-shaped member. A jig can be hooked into the groove to make it easier to attach to or remove from the cradle.
  • the detaching tool of the present invention is a detaching tool for detaching the sample pressing portion corresponding to the detaching means of the sample holder tip portion of the present invention. That is, for example, when the desorption means is a groove, a desorption tool having a dedicated collet that is caught in the groove can be exemplified.
  • the sample pressing portion has a ring shape, it can be a removal tool having a ring-shaped collet that can be hooked in the groove on the inner side of the sample pressing portion cylinder.
  • the kit of the present invention is characterized by comprising the tip of the sample holder of the present invention and the detaching tool of the present invention.
  • Examples of the sample holder tip of the present invention include those described above. Moreover, what was mentioned above can also be mentioned as a removal tool of this invention.
  • the sample holder of the present invention is characterized by comprising the tip of the sample holder of the present invention.
  • the tip of the sample holder those described above can be exemplified.
  • the sample holder tip of the present invention is a sample holder tip comprising a sample mounting base, a sample mesh for placing a sample, a sample pressing means for pressing the sample mesh, and a fixing means for fixing the sample pressing means.
  • the said sample pressing means has an elastic member, It is characterized by the above-mentioned.
  • a sample mesh is placed on the sample mounting base, and the sample is placed on the sample mesh.
  • the sample mesh is usually fixed when used in a microscope.
  • the sample mesh is generally fixed to the sample mounting base with screws or the like through the sample pressing plate.
  • the sample pressing means has an elastic member.
  • the sample pressing means can start to tilt and create a space in which the sample can be taken in and out only by loosening the fixing means for fixing the sample pressing means. Therefore, there is an advantageous effect that the space can be used in a simple and reliable manner in comparison with the conventional method.
  • the elastic member is a hook.
  • the elastic member is not particularly limited as long as the space can be created. From the viewpoint of easy design, examples of the elastic member include a hook and a spring. It should be noted that if the fixing means for fixing the sample pressing means is loosened, any structure can be used as long as the sample pressing means can be lifted and shifted to both sides. For example, a space can be directly formed in the sample pressing means. Even if an elastic member such as a hook or a spring is not attached, the elastic member may be arranged on the cradle side. Therefore, in another embodiment of the present invention, an elastic member can be provided on the sample mounting base side. The elastic member assists the operation such as tilting of the sample pressing means by loosening the fixing means for fixing the sample pressing means, so that an appropriate space can be formed in the region where the sample is inserted.
  • the sample pressing means may be composed of one or more. This is because, even if there is one sample holding means or a plurality of sample pressing means, it is possible to create the above-mentioned space and to perform sample taking in and out much more easily and reliably than in the past.
  • the sample pressing means is housed in a groove provided in the sample setting base.
  • the sample pressing means does not rotate because it fits into the groove at the tip of the sample holder. Since the sample pressing means does not rotate, there is an advantage that the sample is not damaged (bent, contacted with the surface, etc.).
  • the sample pressing means is movable in the longitudinal direction of the sample holder.
  • the sample pressing means By allowing the sample pressing means to move, the sample can be taken in and out more smoothly due to a synergistic effect with the space. If an appropriate space is created between the sample pressing means and the sample mounting base and the sample pressing means moves, the sample is set at a desired position, and then the sample pressing means is moved to the original position. By fixing at a desired position by the fixing means, the sample can be set more reliably without damaging the sample.
  • the sample pressing means is movable, the sample can be taken in and out more smoothly due to a synergistic effect with the space.
  • the sample pressing means may have a guide groove.
  • the sample pressing means When the sample pressing means is moved using the guide groove as described above, the sample pressing means can be easily slid in the lateral direction using, for example, tweezers, and the sample can be taken in and out. It becomes possible to make it easy.
  • the sample holder of the present invention is characterized by comprising the tip of the sample holder of the present invention.
  • the tip of the sample holder those described above can be exemplified.
  • the gonio stage of the present invention includes a gate type valve, a guide roller provided in the gate type valve, a first vacuum O-ring provided in the gate type valve, and the gate type valve driving shaft.
  • a valve opening / closing mechanism comprising the valve opening / closing mechanism, wherein the gate valve and the shaft are rotatable by at least one fulcrum.
  • the gate type valve is a valve that can open and close between a sample observation chamber (usually high vacuum) of an electron microscope and a preliminary exhaust chamber.
  • the gate type valve can be designed to move so that the gate type valve can be opened and closed in accordance with the movement of the gate type valve driving shaft.
  • the guide roller provided in the gate type valve is provided so that the valve can be easily opened and closed.
  • the guide roller provided in the gate type valve is not essential, the presence or absence of the guide roller makes it possible to open and close the valve more smoothly than when there is no guide roller. In addition, it does not specifically limit about the number of guide rollers, When installing, you may provide one or more guide rollers.
  • the first vacuum O-ring provided in the gate type valve is for accurately shutting off the sample observation chamber (high vacuum) of the electron microscope and the preliminary exhaust chamber.
  • the gate type valve When the gate type valve is set at a position where the valve is closed, the O-ring can seal between the sample observation chamber of the electron microscope and the preliminary exhaust chamber by high vacuuming.
  • the gate valve driving shaft is rotatably connected to the gate valve.
  • the gate valve and the shaft can be rotated by at least one fulcrum of the gate valve and the shaft.
  • the gate type valve can be rotated around the axis about a direction substantially perpendicular to the longitudinal direction of the shaft.
  • the shaft can be gradually bent from the horizontal state to an angle of 90 degrees by moving the shaft in the direction of the sample observation chamber of the electron microscope (the direction of the center of the electron microscope). Is possible.
  • the guide roller, the support roller, the taper portion, and the like provided on the gate valve can open and close the valve more smoothly.
  • the axial direction of the fulcrum is parallel to the opening / closing surface of the valve. This is because when the valve is closed in such a manner that the gate type valve covers the high vacuum side cylinder on the opening / closing surface, the opening / closing is performed more accurately.
  • the valve opening / closing mechanism has a support roller.
  • the valve opening / closing mechanism has a tapered portion for guiding the guide roller.
  • the gate type valve can be easily introduced into a predetermined position or pulled out from the bookstore position according to the inclination. It is also possible to open and close the gate type valve more accurately.
  • the support roller and taper can support smooth operation even when the valve is opened.
  • the angle can be changed so that the gate type valve and the shaft are substantially in a straight line.
  • the valve can be in a fully open state in a substantially straight line.
  • a guide roller, a support roller, a taper part, etc. it supports so that opening and closing of a valve can be performed more smoothly than those without these.
  • the shaft when the shaft extends in the substantially central direction of the electron microscope tube (when the longitudinal direction of the shaft is the substantially central direction of the pupil microscope tube), the direction perpendicular to the central axis direction of the electron microscope tube
  • the shaft can be movable.
  • the gate type valve and the shaft are closed by an elastic member, for example, a spring, and the gate type valve is closed, that is, the gate type valve and the shaft are approximately 90 degrees (the valve opening and closing surface is approximately the axis of the microscope tube).
  • the shaft if the shaft is set so that the longitudinal direction is substantially perpendicular to the microscope tube, the shaft can be moved toward the sample observation chamber.
  • the gate type valve can change the angle and smoothly close the valve through at least one fulcrum of the valve and the shaft.
  • the shaft has a second vacuum O-ring. This is used to block the preliminary exhaust chamber from the outside when performing preliminary exhaust (preliminary evacuation). Even if it is not the second vacuum O-ring, it is not particularly limited as long as it can be shut off from the outside by means of the same.
  • the shaft itself may have a blockable member, or a vacuum O-ring or the like may be provided on the sample holder holding cylinder side.
  • the shaft is in a shaft holding cylinder in a sample holder holding cylinder.
  • the shaft may be integrally formed and incorporated in the sample holder holding cylinder, or may be separately incorporated into the shaft holding cylinder by forming a shaft holding cylinder.
  • the shaft is not particularly limited as long as it can move to open and close the valve.
  • the sample holder holding cylinder has a sample holder holding member.
  • the sample holder holding member has a role of holding the sample holder in the preliminary exhaust state position of the sample holder.
  • Examples of the sample holder holding member include a hook. If the sample holder holding member is held together, after the preliminary evacuation is completed, the gate type valve is opened remotely, and the sample holder holding member, for example, the hook is remotely operated to reserve the sample holder. The evacuation process and the sample holder insertion process can be performed remotely. Thereby, once the sample holder is mounted on the gonio stage, it can be quickly removed from the electron microscope room, so that the disturbance of the environment of the electron microscope room can be minimized. Furthermore, when a cooled sample holder is used, a dangerous accident of overflowing liquid nitrogen can be avoided.
  • FIG. 1 (a) is a cross-sectional view showing a state in which a sample is attached when the sample holder tip is used in one embodiment of the present invention.
  • FIG. 1 (b) shows a cross-sectional view after completion of sample attachment when the sample holder tip is used in one embodiment of the present invention.
  • reference numeral 1 denotes a detaching tool, and in this example, a sample pressing ring mounting jig. The state of the collet holding the sample pressing ring is shown.
  • Reference numeral 2 denotes a sample pressing portion, which is a sample pressing ring in this example.
  • 3 is a sample mesh
  • 4 is a sample holder shaft portion
  • 5 is a detaching means (a groove in this case) for detaching the sample pressing portion
  • 6 is a sample mounting base (cradle body)
  • 7 is a link for giving a cradle inclination
  • 8 Denotes a cradle support pivot pin
  • 9 denotes a sample holder tip (pivot support frame portion).
  • Reference numeral 10 denotes a detaching tool.
  • a sample pressing ring mounting jig is shown. It shows a normal state without collet expansion.
  • Reference numeral 11 denotes a rod of the collet opening mechanism of the sample pressing ring mounting jig.
  • the sample mesh can be fixed to the tip of the sample holder by sandwiching the sample mesh 3 with the collet expanded and the ring 2 held.
  • the collet is narrowed by pulling out the rod 11, and the fixation between the ring 2 and the mounting jig is released.
  • the ring 2 is clamped by the clamp portion and fixed to the tip end portion of the sample holder.
  • FIG. 2 is a view showing a sample holder tip in one embodiment of the present invention.
  • 20 is a detaching tool (sample pressing ring mounting jig)
  • 21 is a collet part of the sample pressing ring mounting jig
  • 22 is a sample pressing part (sample pressing ring)
  • 23 is a sample mesh
  • 24 is a clamping part (sample pressing ring).
  • clamp bar spring of ring 25 is a sample mounting base
  • 26 is a pivot support frame portion
  • 27 is a cradle support pivot pin
  • 28 is a rod of a collet portion opening mechanism of a sample pressing ring attachment jig
  • 29 is a force point for tilting the cradle
  • 30 is a link for providing a cradle inclination
  • 31 is a return spring plate
  • 32 is a sample holder shaft.
  • the mounting jig 20 fixes the ring 22 to the tip of the sample holder via the sample mesh 23 in a state where the ring 22 is fixed. Thanks to the taper provided on the ring 22, it engages with the clamp portion 24, and the ring 22 is fixed to the tip of the sample holder.
  • the ring 22 and the clamp portion 24 are fixed at two locations, but may be fixed at one location or a plurality of locations.
  • FIG. 3A shows a conventional standard cradle.
  • FIG. 3B is a diagram showing a cradle in one embodiment of the present invention.
  • FIG. 4 is a schematic diagram of a cradle using a conventional sample pressing plate and fixing screws.
  • FIG. 4 is an enlarged view of FIG. 3 and 4, reference numeral 40 denotes a fixing screw for holding the sample, 41 denotes a ⁇ tilt movable range, 42 denotes a ⁇ tilt pivot position, 43 denotes an upper pole piece of the objective lens, 44 denotes a sample pressing plate, and 45 denotes a link for a tilt driving force point. , 46 denotes a sample cradle, and 47 denotes a lower pole piece of the objective lens.
  • the ⁇ tilt movable range is limited due to the presence of the screw 40 or the like.
  • the tip of the sample holder of the present invention has a more compact design in terms of thickness and width, and the ⁇ tilt movable range is greatly expanded, so that it is expected that more information can be obtained from the sample.
  • the sample holder having the sample holder tip of the present invention is actually capable of obtaining more information from the sample by expanding the ⁇ tilt movable range as shown in FIG. 3B. It has been found.
  • FIG. 5 is a diagram showing a procedure for attaching the tip of the sample holder in one embodiment of the present invention.
  • 51 is a schematic view from a state where the fixing means is loosened to a state where the fixation is loosened
  • 52 is a schematic view where the specimen holding means is moved from a state where the fixation is loosened
  • 53 is a sample.
  • Direction of movement of the holding means 54 is a guide groove
  • 55 is a space for movement (groove)
  • 56 is a groove provided on the sample mounting base
  • 57 is a fixing means
  • 58 is a sample holder body
  • 59 is a sample
  • 60 is a sample holder.
  • Means, 61 is an elastic member
  • 62 is a sample mounting base (cradle body).
  • a sample attachment procedure in one embodiment of the present invention will be described as follows. First, referring to FIGS. 5 and 6, by loosening the fixing means 57 for fixing the sample pressing means 60, the fixing of the sample mesh and the sample spacer for placing the sample can be released, although not shown. it can.
  • a screw is used as the fixing means 57, but is not particularly limited as long as the sample pressing means 60 can be fixed. If the fixing of the fixing means 57 is loosened, the sample pressing means 60 has the elastic member 61, so that the sample pressing means 60 is gradually inclined to create a space above the position where the sample is placed.
  • the elastic member 61 provided in the sample pressing means 60 serves as a spring and lifts the sample pressing means, thereby forming a space.
  • a hook is used as the elastic member, but it is needless to say that the hook is not particularly limited thereto.
  • the tip of a tweezers or the like is inserted into the guide groove 54 using the guide groove 54 provided in the sample pressing means 60, as indicated by an arrow 53 in FIG. Can be opened on both sides.
  • two sample pressing means are arranged symmetrically, but there may be one or more than one, and there is no particular limitation as long as a space is formed.
  • the sample pressing means 60 When the sample is set, when the sample pressing means 60 is fixed by the fixing means 57 or when the sample pressing means 60 is moved, the guide groove 54 is used again and the tip of tweezers or the like is placed in the guide groove 54. Then, the sample pressing means 60 is slid and moved inward as indicated by an arrow 53 in FIG. Thereafter, the sample pressing means 60 can be fixed by the fixing means 57 to fix the sample. In the figure, since a screw is used as a fixing means, fixing the sample is completed when the screw is tightened.
  • the elastic member such as a hook
  • the sample pressing means can self-react by simply loosening the fixing means such as a screw. Since the sample is lifted, the sample may be set as it is, and if necessary, the sample can be attached to the sample holder by simply moving the sample pressing means.
  • FIG. 7 is a diagram showing a perspective view of the tip end portion of the sample holder in one embodiment of the present invention.
  • the guide groove penetrates the sample pressing means, but if the sample pressing means can be moved, it does not need to penetrate.
  • a hook is used as the elastic member.
  • one or more elastic members on the lingual side of the sample pressing means at an appropriate location, immediately above the sample installation position, A space can be formed in the sample, and the sample can be prevented from being damaged when the sample is installed.
  • the present invention has the following merits and characteristics.
  • the sample pressing means is lifted simply by loosening the fixing means such as screws, a space is created between the sample pressing means and the sample mounting base, and the sample can be detached. Further, it was found that the portion for holding the sample is floating, and the sample holding means does not hit the surface of the sample or damage the sample mesh by hitting it from the side. Further, it has been found that it is not necessary to place the sample again and again because the sample can be attached smoothly (improved working efficiency) and simplified. By simplifying the work, there is an effect of reducing accidents due to mounting errors such as sample breakage. Furthermore, since the working time can be shortened, it has been found that there is also a synergistic effect that the contamination on the sample can be reduced.
  • the electron microscope of the present invention has the goniostage of the present invention described above in the third aspect.
  • the electron microscope is not particularly limited.
  • the gonio stage and the electron microscope of one embodiment of the present invention will be described with reference to the drawings, but the present invention is not intended to be limited to these.
  • FIG. 10 shows a conceptual diagram of a basic configuration in an example of a transmission electron microscope applicable in the present invention.
  • 101 is a vacuum region part
  • 102 is an electron acceleration electrode
  • 103 is an insulating gas region
  • 104 is an X-ray absorbing member
  • 105 is a condenser diaphragm (movable mechanism part)
  • 106 is an objective diaphragm (movable mechanism part)
  • 107 Is a field limiting diaphragm (movable mechanism)
  • 108 is a second intermediate imaging lens
  • 109 is a projection lens
  • 110 is an observation glass window
  • 111 is a fluorescent screen
  • 112 is an image acquisition camera
  • 113 is a camera room
  • 114 is a vacuum Partition valve
  • 115 is a first intermediate imaging lens
  • 116 is a back focus lens
  • 117 is an objective (lower pole) lens
  • 118 is an objective (upper pole) lens
  • 119 is a second convergen
  • 125 denotes a coil member for an electron beam deflector or astigmatism corrector
  • 126 denotes a coil member for each converging electron lens. It is possible to incorporate the goniostage of the present invention into an electron microscope according to such an example.
  • FIG. 11 shows a gonio stage according to an example of the present invention.
  • the state when the gate type valve is closed is shown.
  • FIG. 13 shows an embodiment of a gonio stage in an example of the present invention.
  • the state when the gate type valve is opened is shown.
  • 11 and 13 131 is a vacuum side, 132 is a gate type valve block, 133 is a vacuum seal O-ring, 134 is a mounting position of an elastic member for gate type valve block, and 135 is an elastic member for gate type valve block.
  • Detachment prevention pin, 136 and 137 are gate type valve block lifting support rollers, 138 is a vacuum seal O-ring, 139 is a sample holder holding cylinder, 140 is a gate type valve block driving shaft, 141 is a sample holder insertion side, Reference numeral 142 denotes a frame and sample holder holding cylinder of a gate type valve block lifting support roller, 143 denotes a route guide roller, 144 denotes a fulcrum, 145 denotes a tapered portion, and 146 denotes a preliminary exhaust chamber.
  • the shaft is shown on the upper side, but since the same effect is obtained regardless of whether the shaft is installed on the lateral side, the lower side or the like, the position of the shaft or the like is not limited.
  • FIG. 12 shows a gonio stage according to an example of the present invention.
  • the movement of opening and closing the gate type valve is shown.
  • the trajectory of the opening and closing movement is depicted step by step.
  • 151 is the fulcrum closed position
  • 152 is the fulcrum open position
  • 153 is the opening / closing piston rod stroke distance
  • 154 is the O-ring position (the O-ring position of the gate type valve opening / closing shaft is the gate type valve opened) It is indicated by the position).
  • the valve is normally closed as shown in FIG.
  • the sample holder is inserted up to the preliminary exhaust chamber 146.
  • the valve is still closed.
  • a sample holder holding member for example, a hook (not shown) is installed so that the tip of the sample holder stops once it is not in contact with a valve or the like (not shown)
  • the sample holder is placed at a position corresponding to the sample holder holding member. If a groove or the like is provided on the side, the sample holder temporarily stops.
  • the shaft 140 can be pulled out or inserted by an actuator or the like, and can be automated by computer control. That is, it is possible by computer control to pull out the shaft and open and close the valve simultaneously with the signal that the preliminary exhaust is finished.
  • a signal to release the sample holder from the holding member causes the sample holder to be released from the state temporarily fixed by the holding member and pulled into the high-vacuum electron microscope. . In this way, sample observation becomes possible.
  • the shaft can be automatically moved by an air pist, an actuator or the like so as to close the gate type valve.
  • the fixing of the sample holder by the holding member can also be automatically released.
  • the present invention since the misoperation and the time until the start of observation can be shortened particularly when the sample holder for the cooled sample is inserted, the throughput is improved and the productivity is improved. Further, it has been found that the present invention also has an advantage that the atmosphere in the electron microscope chamber is stabilized by auto conversion.
  • Such a sample holder tip of the present invention according to the first and second aspects can cope with various human errors and has an advantageous effect even in combination with other devices. It can be expected to be useful in a wide range of fields.
  • the misoperation at the time of inserting the sample holder of the cooled sample and the time until the start of observation can be shortened, the throughput is improved and the productivity is improved.
  • Auto makes the atmosphere inside the electron microscope stable and contributes to the improvement of analysis capabilities, such as shortening the data acquisition time and improving the quality of analysis data, and can be applied in a wide range of technical fields.
  • Example holding ring mounting jig. Cold holding the sample holding ring
  • Sample holder sample holder ring
  • Sample mesh 4 Sample holder shaft
  • Desorption means for detaching the sample holder
  • Sample mounting base cradle body
  • Links giving cradle tilt Cradle support pivot pin
  • Sample holder tip pivot support frame
  • Detachment tool (Sample holding ring mounting jig. (Normal state without expansion of collet)) 11.
  • Rod 20 for collet opening mechanism of sample pressing ring mounting jig Desorption tool (sample pressing ring mounting jig) 21 Collet part of sample pressing ring mounting jig 22 Sample pressing part (sample pressing ring) 23 Sample mesh 24 Clamp part (Clamp bar spring of sample holding ring) 25 Sample installation base 26 Pivot support frame portion 27 Cradle support pivot pin 28 Rod of collet portion opening mechanism 29 of sample pressing ring attaching jig 29 Cradle tilt force point receiving portion 30 Cradle tilt link 31 Push-back spring plate 32 Sample holder shaft portion 40 Sample holding screw 41 ⁇ tilt movable range 42 ⁇ tilt pivot position 43 Objective lens upper pole piece 44 Sample holding plate 45 Tilt driving force point link 46 Sample cradle 47 Objective lens lower pole piece 51 Fixed by fixing means Fig.
  • FIG. 52 is a schematic view from a state where the fixing is loosened.
  • Fig. 52 is a schematic diagram when the sample pressing means is moved from a state where the fixing is loosened.
  • 53 A moving direction of the sample pressing means 54
  • a guide groove 55 A space for movement (groove) 56 Groove 57 provided on the sample mounting base 57
  • Fixing means 58 Sample holder main body 59
  • Sample 60 Sample holding means 61
  • Elastic member 62
  • Sample mounting base (cradle main body) 70 Schematic diagram showing a state in which the sample presser is moved in the direction of the arrow from a state in which the sample is set 71
  • 81 Sample mesh 82
  • Sample Spacer 101 Vacuum region 102
  • Electron accelerating electrode 103
  • Insulating gas region 104
  • X-ray absorbing member 107
  • Field-limiting aperture

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

L'objet de la présente invention est de fournir une partie d'extrémité de porte-échantillon permettant d'échanger en toute sécurité des échantillons dans un microscope électronique. La partie d'extrémité de porte-échantillon est composée : d'un siège de pose d'échantillon (6) ; d'une maille pour échantillon (3) destinée à porter un échantillon ; d'une partie de retenue d'échantillon (2) destinée à retenir la maille pour échantillon (3) ; et d'une partie de serrage (24) qui serre la partie de retenue d'échantillon (2).
PCT/JP2013/004315 2012-07-17 2013-07-12 Partie d'extrémité de porte-échantillon, porte-échantillon présentant ladite partie d'extrémité de porte-échantillon, étage gonio et microscope électronique présentant ledit étage gonio WO2014013709A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US14/414,682 US9240304B2 (en) 2012-07-17 2013-07-12 Specimen holder tip part, specimen holder having said specimen holder tip part, gonio stage, and electron microscope having said gonio stage

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2012158550A JP5908357B2 (ja) 2012-07-17 2012-07-17 ゴニオステージ、及び当該ゴニオステージを有する電子顕微鏡
JP2012-158550 2012-07-17
JP2012214258A JP6137801B2 (ja) 2012-09-27 2012-09-27 試料ホルダー先端部、及び前記試料ホルダー先端部を有する試料ホルダー
JP2012-214258 2012-09-27

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JP6127191B1 (ja) * 2016-10-03 2017-05-10 株式会社メルビル 試料ホルダー
JP6906786B2 (ja) * 2017-03-27 2021-07-21 株式会社日立ハイテクサイエンス 試料保持具、部材装着用器具、および荷電粒子ビーム装置
CN107315020B (zh) * 2017-07-31 2023-08-04 中国科学院宁波材料技术与工程研究所 一种透射电子显微镜样品杆的原位芯片固定结构
JP6995099B2 (ja) * 2019-09-30 2022-01-14 日本電子株式会社 試料取付装置
CN110933321B (zh) * 2019-12-31 2021-03-09 重庆盛泰光电有限公司 一种双摄像头摄像模组
JP7127087B2 (ja) * 2020-07-15 2022-08-29 日本電子株式会社 透過電子顕微鏡および対物絞りの調整方法
EP4047632B1 (fr) * 2021-02-23 2023-08-09 Bruker AXS GmbH Outil pour des applications de grille de microscopie à transmission électronique (met)
US11996264B1 (en) * 2023-09-06 2024-05-28 Honeywell Federal Manufacturing & Technologies, Llc Sample mount for electron backscatter diffraction

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